CN108144556A - A kind of boiling bed hydrogenation reaction system and boiling bed hydrogenation technique method - Google Patents
A kind of boiling bed hydrogenation reaction system and boiling bed hydrogenation technique method Download PDFInfo
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- CN108144556A CN108144556A CN201810107890.4A CN201810107890A CN108144556A CN 108144556 A CN108144556 A CN 108144556A CN 201810107890 A CN201810107890 A CN 201810107890A CN 108144556 A CN108144556 A CN 108144556A
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- 238000005984 hydrogenation reaction Methods 0.000 title claims abstract description 53
- 238000009835 boiling Methods 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000003054 catalyst Substances 0.000 claims abstract description 100
- 239000001257 hydrogen Substances 0.000 claims abstract description 45
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 45
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 44
- 238000007599 discharging Methods 0.000 claims abstract description 9
- 239000012071 phase Substances 0.000 claims description 77
- 239000007788 liquid Substances 0.000 claims description 42
- 239000007789 gas Substances 0.000 claims description 23
- 238000006243 chemical reaction Methods 0.000 claims description 21
- 230000008602 contraction Effects 0.000 claims description 19
- 239000000463 material Substances 0.000 claims description 18
- 239000002994 raw material Substances 0.000 claims description 12
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 9
- 239000012295 chemical reaction liquid Substances 0.000 claims description 8
- 238000012545 processing Methods 0.000 claims description 7
- 238000010276 construction Methods 0.000 claims description 6
- 239000007791 liquid phase Substances 0.000 claims description 6
- 238000011068 loading method Methods 0.000 claims description 6
- 238000005192 partition Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 4
- 229910052750 molybdenum Inorganic materials 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 229910052721 tungsten Inorganic materials 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 20
- 238000004939 coking Methods 0.000 abstract description 8
- 238000005516 engineering process Methods 0.000 abstract description 5
- 230000006641 stabilisation Effects 0.000 abstract description 2
- 238000011105 stabilization Methods 0.000 abstract description 2
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 239000011949 solid catalyst Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000001154 acute effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000011344 liquid material Substances 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000003321 amplification Effects 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000011280 coal tar Substances 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 239000003027 oil sand Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000000819 phase cycle Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000003079 shale oil Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/1818—Feeding of the fluidising gas
- B01J8/1827—Feeding of the fluidising gas the fluidising gas being a reactant
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/005—Separating solid material from the gas/liquid stream
- B01J8/007—Separating solid material from the gas/liquid stream by sedimentation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/1809—Controlling processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/1845—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with particles moving upwards while fluidised
- B01J8/1863—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with particles moving upwards while fluidised followed by a downward movement outside the reactor and subsequently re-entering it
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/20—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium
- B01J8/22—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium gas being introduced into the liquid
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G45/00—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds
- C10G45/02—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing
- C10G45/14—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing with moving solid particles
- C10G45/20—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing with moving solid particles according to the "fluidised-bed" technique
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G47/00—Cracking of hydrocarbon oils, in the presence of hydrogen or hydrogen- generating compounds, to obtain lower boiling fractions
- C10G47/24—Cracking of hydrocarbon oils, in the presence of hydrogen or hydrogen- generating compounds, to obtain lower boiling fractions with moving solid particles
- C10G47/30—Cracking of hydrocarbon oils, in the presence of hydrogen or hydrogen- generating compounds, to obtain lower boiling fractions with moving solid particles according to the "fluidised-bed" technique
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Combustion & Propulsion (AREA)
- General Chemical & Material Sciences (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
Abstract
The invention belongs to hydrogen addition technology fields, and in particular to a kind of boiling bed hydrogenation reaction system and boiling bed hydrogenation technique method.The part pipeline coking problem that catalyst discharging system brings by intermittently operated can effectively solve the problem that by one aspect of the present invention, on the other hand the utilization rate (improving catalyst in reactor reserve) of reactor can be further improved, so as to further promote hydrogenation reaction effect, improve the stability of device operation, particularly go into operation, stop work, unusual service condition when can maintain the fluidized state of catalyst stabilization.
Description
Technical field
The present invention relates to a kind of boiling bed hydrogenation reaction system and boiling bed hydrogenation technique methods, belong to hydrogen addition technology neck
Domain.
Background technology
Boiling bed hydrogenation reaction refers to feedstock oil (predominantly liquid phase), hydrogen (gas phase) carries out adding hydrogen on catalyst (solid phase)
The process of reaction, hydrogenation reaction mainly occur hydrodesulfurization, hydrodenitrogeneration, hydrogenation deoxidation plus hydrogen saturation, are hydrocracked.Instead
Device is answered to be operated under the fluidized state of gas, liquid, solid three-phase, catalyst is in the feedstock oil entered from reactor bottom and the band of hydrogen
Under dynamic, in fluidized state, entirely different fluid state is in fixed bed reactors.Boiling bed hydrogenation reaction can be handled
The inferior feedstock oil of high metal, high asphalt content, reaction is with pressure drop is small, temperature is uniform, can add row's catalyst online
The features such as to keep catalyst activity.
Boiling bed hydrogenation reactor will generally set catalyst to add heat-extraction system online, for the addition and discharge of catalyst.
But catalyst adds heat-extraction system to be not continuous use online, and catalyst updating is carried out when usually reactivity worth does not reach requirement,
According to feedstock property and conversion level requirement, general one week or longer time progress catalyst updating it is primary.Under such conditions,
The oil and catalyst of meeting depositing dosed quantities, exist, and part pipeline exists without hydrogen in the pipeline of catalyst discharge system
Under hot conditions (the particularly part of inside reactor), therefore the easy coking of material in this part pipeline, it can be made when serious
It is blocked into pipeline.The prior art does not have suitable solution, generally according to device actual conditions, accumulates operating experience, control
Catalyst updating operation is carried out before pipeline blocks, blocking is avoided to cause plant failure, as a result, causing to be not required to carry out sometimes
During catalyst updating, operation must be also updated by flow, catalyst waste and operating cost is caused to increase.
Presently, there are two kinds of major type of boiling hydrogen addition technologies：
One kind is by the way of oil phase cycle, and such as USRe25, the boiling bed process described in 770, this technique is in reality
Deficiency in is：To keep solid-liquor separation effect, catalyst in reactor dosage cannot be too many, reactor utilization rate
Low, industrial fluidized bed reactor utilization rate generally only 40% or so --- utilization rate refers generally to loaded catalyst and accounts for reactor
The percentage of volume (disregarding end socket space), fixed bed reactors utilization rate general more than 90%；Reactor has larger space to make
Residence time of the liquid material under no catalytic condition is long, this position does not have hydrogenation reaction, and material is easily anti-at high temperature
Answer coking.
Another kind of is that three phase separator is set in reactor, carries out gas-liquid-solid separation in reactor internal upper part, such as
The fluidized bed reactor that CN02109404.7 is introduced, the three phase separator as built in the program by setting can improve catalyst
Dosage, that is, that improves reactor utilizes space, but in actual use, catalyst amount improve it is limited, if catalyst is used
Amount increases, the separating effect rapid decrease of three phase separator, is actually improved than first kind fluidized bed reactor utilization rate limited；
Above-mentioned technology is further improved in CN200710012680.9, sets guide frame in three phase separator lower part, utilizes
Guide frame increases the operating flexibility of three phase separator, it is ensured that three phase separator efficiently separates, and reduces taking out of for catalyst
Amount improves catalyst inventory, improves reactor utilization rate, but when in use, still need to set in three phase separator lower part certain area
Catalyst lean phase region (as shown in its attached drawing, the region catalytic amount is seldom, and hydrogenation reaction does not occur substantially) is put, otherwise three-phase separate
Separating effect from device cannot still be met the requirements, and the presence of dilute-phase zone, influence reactor utilization rate it is further promoted (although
It can be the 40%~70% of reactor volume that catalyst loading amount in reactor shell is pointed out in its specification, but it is general also only
Having can be with steady running in the case of 50% or so), hydrogenation reaction effect is also influenced, and after the amplification of reactor scale, urge
Agent loading amount is more difficult to improve, it is difficult to achieve the effect that experimental provision.
Although the latter is theoretically not required to recycle oil, go into operation, stop work, operation exception when catalyst can be caused to be difficult to reach
Stable fluidized state, operational stability are insufficient.
Invention content
The technical problem to be solved by the present invention is to：Overcome deficiency of the prior art, a kind of boiling bed hydrogenation reaction is provided
On the one hand system and boiling bed hydrogenation technique method can effectively solve the problem that the part that catalyst discharging system is brought by intermittently operated
On the other hand pipeline coking problem can further improve the utilization rate (improving catalyst in reactor reserve) of reactor,
So as to further promoted hydrogenation reaction effect, improve device operation stability, particularly go into operation, stop work, unusual service condition when
It can maintain the fluidized state of catalyst stabilization.
Boiling bed hydrogenation reaction system of the present invention, including boiling bed hydrogenation reactor and catalyst discharging system,
The bottom of reactor shell be equipped with feed(raw material)inlet (raw material include liquid charging stock oil and hydrogen), top be equipped with catalyst add in mouth,
Gas vent and liquid outlet, the top setting gas, liquid, solid three phase separator in reactor cylinder body, bottom setting gas-liquid are distributed
Disk, the region between three phase separator and gas-liquid partition tray are reaction zone, and catalyst discharging system includes the outer row pipeline of catalyst
It is received with outer row's catalyst and reaction zone is stretched into processing system, one end of the outer row pipeline of catalyst below reactor shell
Lower part, the other end is received with outer row's catalyst and processing system connects；Cycle hydrogen system is added, cycle hydrogen system includes recycle hydrogen
Compressor, the isolated hydrogen-containing gas of three phase separator is flowed out through gas vent and reacted gas phase effluent piece-rate system
Circulating hydrogen compressor is passed through, the outlet of circulating hydrogen compressor passes through branch one, branch two and reactor feed system, catalysis respectively
The outer row pipeline of agent connects, and control valve is set on branch two.
Preferably, liquid discharge tube line is set in the liquid phase region of three phase separator, and the outlet of liquid discharge tube line is reaction
The liquid outlet of device cylinder, outlet of the isolated liquid of three phase separator through liquid discharge tube line are passed through reaction liquid phase outflow
Object piece-rate system.Reactor is exported by the liquid that liquid discharge tube line generates hydrogenation reaction.
Preferably, the setting reaction liquid phase effluent circulatory system, the reaction liquid phase effluent circulatory system include circulating pump, follow
The entrance pipe of ring pump is connected with liquid discharge tube line, and the outlet of circulating pump is entered by pipeline and the raw material of reactor shell bottom
Mouth connection.
Preferably, the three phase separator include inner cylinder and outer barrel, inner cylinder and outer barrel are concentric and internal diameter is different, inner cylinder and
The upper/lower terminal of outer barrel is all open, and the upper end opening of outer barrel is less than the upper end opening of inner cylinder, and the lower ending opening of outer barrel is less than
The lower ending opening of inner cylinder；Outer barrel top is direct tube section, and outer barrel lower part is a taper type contraction section, and the lower ending opening of the contraction section is
The lower ending opening of outer barrel；There is spacing, in order to which material passes through between the lower ending opening of inner cylinder and outer barrel contraction section.
It is further preferred that three phase separator is concentric setting with reactor shell, the outer barrel of three phase separator passes through
First support construction is fixed on the inner wall of reactor shell, and the inner cylinder of three phase separator is fixed on outside by the second support construction
On the inner wall of cylinder.
In practical application, the contraction pars infrasegmentalis of outer barrel can be designed as direct tube section in three phase separator, i.e. outer barrel is from upper
Direct tube section-contraction section-straight tube segment structure is followed successively by under.Wherein, a diameter of reactor shell internal diameter of outer barrel top direct tube section
50%~90%, preferably 75%~85%；Annular space distance between inner cylinder and outer barrel is outer barrel corresponding position radius
30%~70%, preferably 40%~60%；The difference in height of inner cylinder upper end and outer barrel upper end is the 10%~50% of outer barrel radius,
Preferably 20%~40%；Spacing between the lower ending opening of inner cylinder and outer barrel contraction section for outer barrel direct tube section radius 5%~
40%, preferably 10%~30%；The 10%~50% of a diameter of outer barrel direct tube section diameter of outer barrel contraction section lower ending opening, preferably
It is 15%~35%；The angle of throat (acute angle of direct tube section and taper type contraction section) of outer barrel lower part taper type contraction section is
20 °~80 °, preferably 30 °~60 °；The height of outer barrel top direct tube section is 0.4~3m, preferably 0.5~1m.
In reactor cylinder body, the top setting gas-phase space of three phase separator, the height of gas-phase space is reactor cylinder
The 0~20% of body (not including reactor end socket part), preferably 5%~10%.
Preferably, the lower section setting baffle of the lower ending opening of the outer barrel of three phase separator, baffle can be upper and lower two
Hold spindle small, broad in the middle, 1~3 times of a diameter of outer barrel lower ending opening diameter of spindle axial cross section maximum.It leads
It is set between fluid and three phase separator outer barrel lower port suitable for gap.
In the present invention, other components can be arranged as required in reactor, such as system for detecting temperature, pressure detecting system
The one or more such as system, fluid flow state detecting system, catalyst distribution condition detecting system, material reallocation system.Above-mentioned structure
Part can be determined by those skilled in the art by the prior art.
Entire boiling bed hydrogenation reaction system can also be arranged as required to corollary apparatus, such as raw material pump, heat exchanger, heating
Stove, separator etc..Above-mentioned corollary apparatus can be determined by those skilled in the art by the prior art.
Boiling bed hydrogenation technique method of the present invention has used above-mentioned boiling bed hydrogenation reaction system.Specifically boiling
It rises in bed hydroprocessing process, reaction raw materials use heavy or inferior feedstock oil (such as decompression residuum, coal tar, liquefied coal coil, drip
Green oil-sand, shale oil etc.)；Catalyst is solid particle, and particle diameter (in terms of isometric spherical shape) is 0.6~2mm, catalyst with
Aluminium oxide is carrier, at least one such as Mo, W, Ni, Co for active component, while can add related auxiliaries.Catalyst is anti-
50%~85%, preferably 65%~80% that device interior loading amount (in terms of stationary state) is reactor volume is answered, most preferably
72%~78%.Specific reaction condition can determine that it is 5 to be commonly designed reaction pressure according to feedstock property and reaction depth requirement
~25MPa, reaction temperature are 200~500 DEG C, and hydrogen and feedstock oil standard state lower volume ratio are 300~2000, feedstock oil with
The volume space velocity that catalyst volume (stationary state) is compared is 0.1~2h-1。
Preferably, when hydrogenation reaction is carried out in the reactor of boiling bed hydrogenation reaction system, control loop hydrogen compressor
Control valve between outlet and the outer row pipeline of catalyst on branch two, makes recycle hydrogen accomplished continuously or intermittently by row pipeline outside catalyst
Into in reactor cylinder body, this mode of operation is it is possible to prevente effectively from the outer row pipeline of catalyst the problem of material coking.Further
Preferably, outside catalyst row pipeline enter cycle hydrogen amount in reactor cylinder body for global cycle hydrogen amount 5% hereinafter, it is preferred that
2% hereinafter, most preferably 0.5% hereinafter, make the material flow in the outer row pipeline of catalyst be not less than 0.1 meter per second simultaneously.
The present invention recycles the structure setting of hydrogen system and catalyst discharging system by optimization, and a small amount of recycle hydrogen passes through catalysis
The outer row pipeline of agent enters in reactor cylinder body, by the material push-in reactor in row pipeline outside catalyst, is not influencing normally
Under the premise of operation, efficiently solve the outer row pipeline internal cause material of catalyst and do not flow and be easy to tie under high temperature hydrogen-free operating mode
The problem of burnt, has many advantages, such as simple in structure, easily operated.
Meanwhile show to influence the factor of three phase separator separating effect in fluidized bed reactor by largely furtheing investigate
It is not only in that structure, the material system status of three phase separator, also has much relations with earth rotation.In fluidized bed reactor
Gas, liquid, solid three-phase state, for gas, liquid generally in the state that flows up, solid catalyst is in boiling quick condition.The earth
Rotation has certain active force to above-mentioned material state, forms slight cyclonic action, in the larger reactor of industry, due to
Larger, this cyclonic action more shows.As a result, catalyst is more assembled in the region close to reactor wall, instead
Answer device radial center region more sparse.This effect produces the separating effect of existing three phase separator and significantly affects, i.e.,
When loaded catalyst increase, the solid catalyst that three phase separator is separated settles back the resistance increase in reactor,
The chance for being taken out of reactor by liquid material improves, and reactor is made to take catalytic amount increase out of.To solve the problems, such as this, usually exist
Three phase separator lower part set catalyst dilute-phase zone, with overcome catalyst sedimentation flow back resistance, but the measure the result is that
Reactor utilization rate reduces, and reaction effect is affected.Before making the present invention, those skilled in the art do not recognize influence
The full content of three phase separator separating effect influence factor in fluidized bed reactor, into without proposing suitable solution party
Case.
The present invention is on the basis of the studies above, for earth rotation to the shadow of flow state in large-scale fluidized bed reactor
It rings, has redesigned novel ebullated bed three phase separator, solved problem of the prior art, further improved the profit of reactor
With rate (improving catalyst in reactor reserve).
The possessed compared with prior art advantageous effect of the present invention is：
1st, when the present invention carries out hydrogenation reaction in the reactor of boiling bed hydrogenation reaction system, control loop hydrogen compressor
Control valve between outlet and the outer row pipeline of catalyst on branch two makes appropriate recycle hydrogen accomplished continuously or intermittently by being arranged outside catalyst
Pipeline enters in reactor cylinder body, this mode of operation is it is possible to prevente effectively from the outer row pipeline of catalyst the problem of material coking.
2nd, it is influenced caused by catalyst distribution unevenness caused by the structure design of three phase separator overcomes earth rotation anti-
Effect problem is answered, meanwhile, the solid catalyst that three phase separator separates is flowed back in reactor radial center regional subsidence
Into reactor, when solving high catalyst loadings, the big problem of resistance of catalyst sedimentation reflux ensure that three phase separator
Still there is good separating effect in high catalyst loadings, it is special so as to further improve loaded catalyst ratio
It is not the Catalyst packing ratio of large-scale industry fluidized bed reactor, while reactor volume utilization rate is improved, reduces
Or catalyst lean phase region is eliminated, improve hydrogenation reaction effect.
Description of the drawings
Fig. 1 is the structure diagram of boiling bed hydrogenation reaction system in the present invention.
In figure：1st, feed(raw material)inlet；2nd, gas-liquid partition tray；3rd, reactor shell；4th, reaction zone；5th, baffle；6th, outer barrel；7、
Inner cylinder；8th, liquid discharge tube line；9th, catalyst adds in mouth；10th, gas vent；11st, gas phase effluent piece-rate system is reacted；12、
Recycle hydrogen system；13rd, liquid phase effluent piece-rate system is reacted；14th, branch one；15th, branch two；16th, control valve；17th, inlet tube
Road；18th, circulating pump；19th, pipeline；20th, outer row's catalyst reception and processing system；21st, the outer row pipeline of catalyst；22nd, reactor
Feed system.
Specific embodiment
The embodiment of the present invention is described further below in conjunction with the accompanying drawings：
Embodiment 1：
Boiling bed hydrogenation reaction system as shown in Figure 1 is used in embodiment 1.In the reaction of boiling bed hydrogenation reaction system
When hydrogenation reaction is carried out in device, the control between the outlet of control loop hydrogen compressor and the outer row pipeline 21 of catalyst on branch 2 15
Valve 16 makes recycle hydrogen accomplished continuously or intermittently enter in reactor shell 3 by row pipeline outside catalyst 21, this mode of operation can have
Effect avoids the problem that material coking in the outer row pipeline 21 of catalyst.Control row pipeline 21 outside catalyst enters reactor shell 3
Interior cycle hydrogen amount is the 0.2% of global cycle hydrogen amount, while the material flow in the outer row pipeline 21 of catalyst is made to be not less than 0.1
Meter per second.
Through experiment, outer 21 long period of row pipeline of catalyst can be kept to keep clear state, i.e. the present embodiment is not influencing
Under the premise of normal operating, efficiently solve the outer 21 internal cause material of row pipeline of catalyst and do not flow and under high temperature hydrogen-free operating mode
The problem of being easy to coking.
Embodiment 2：
The boiling bed hydrogenation reaction system structure used in embodiment 2 is as shown in Figure 1, it includes boiling bed hydrogenation reaction
Device, catalyst discharging system, cycle hydrogen system 12 and the reaction liquid phase effluent circulatory system.
The bottom of reactor shell 3 be equipped with feed(raw material)inlet 1 (raw material include liquid charging stock oil and hydrogen, by reactor into
Material system 22 is fed), top is equipped with catalyst and adds in mouth 9, gas vent 10, and top is equipped with liquid outlet.Reactor cylinder
Top setting gas, liquid, solid three phase separator in body 3, setting liquid discharge tube line 8, liquid in the liquid phase region of three phase separator
Liquid outlet of the outlet of discharge pipe 8 for reactor shell 3, the isolated liquid of three phase separator is through liquid discharge tube line
8 outlet is passed through reaction liquid phase effluent piece-rate system 13, is exported by the liquid that liquid discharge tube line 8 generates hydrogenation reaction
Reactor；Bottom setting gas-liquid partition tray 2 in reactor shell 3；Region between three phase separator and gas-liquid partition tray 2 is
Reaction zone 4；The top setting gas-phase space of three phase separator.
Catalyst discharging system includes the outer row pipeline 21 of catalyst and outer row's catalyst receives and processing system 20, catalyst
One end of outer row pipeline 21 stretches into the lower part of reaction zone 4 from the lower section of reactor shell 3, the other end received with outer row's catalyst and
Processing system 20 connects.
It recycles hydrogen system 12 and includes circulating hydrogen compressor, the isolated hydrogen-containing gas of three phase separator is through gas vent 10
It flows out and reacted gas phase effluent piece-rate system 11 is passed through circulating hydrogen compressor, the outlet of circulating hydrogen compressor passes through respectively
Branch 1, branch 2 15 are connected with reactor feed system 22, the outer row pipeline 21 of catalyst, and control valve is set on branch 2 15
16。
It reacts the liquid phase effluent circulatory system and includes circulating pump 18, entrance pipe 17 and the liquid discharge tube line of circulating pump 18
8 connections, the outlet of circulating pump 18 is connected by pipeline 19 with the feed(raw material)inlet 1 of 3 bottom of reactor shell.
Wherein, three phase separator includes inner cylinder 7 and outer barrel 6, and inner cylinder 7 and outer barrel 6 are with one heart and internal diameter is different, inner cylinder 7 and outer
The upper/lower terminal of cylinder 6 is all open, and the upper end opening of outer barrel 6 is less than the upper end opening of inner cylinder 7, and the lower ending opening of outer barrel 6 is low
In the lower ending opening of inner cylinder 7；6 top of outer barrel be direct tube section, 6 lower part of outer barrel be a taper type contraction section, the lower end of the contraction section
The lower ending opening being open as outer barrel 6；In the present embodiment, the lower part of contraction section is designed as direct tube section, i.e., outer barrel 6 is from top to bottom successively
For direct tube section-contraction section-straight tube segment structure；There is spacing, in order to material between the lower ending opening of inner cylinder 7 and outer barrel contraction section
Pass through.Three phase separator is concentric setting with reactor shell 3, and the outer barrel 6 of three phase separator is consolidated by the first support construction
It is scheduled on the inner wall of reactor shell 3, the inner cylinder 7 of three phase separator is fixed on by the second support construction on the inner wall of outer barrel 6.
The lower section setting baffle 5 of the lower ending opening of the outer barrel 6 of three phase separator, baffle 5 is the spindle that upper and lower ends are small, broad in the middle
Shape.
Three phase separator separating effect carries out simulated experiment using chill.The size of cold model unit is：Reactor shell 3
Internal diameter is 200mm, is highly 3500mm；The height of three phase separator be 400mm, the diameter of 6 top direct tube section of outer barrel
300mm, the annular space distance between inner cylinder 7 and outer barrel 6 is 80mm；The difference in height of 7 upper end of inner cylinder and 6 upper end of outer barrel is 60mm, interior
60mm is in gap between the lower ending opening of cylinder 7 and outer barrel contraction section, a diameter of 90mm of outer barrel contraction section lower ending opening, outer barrel 6
The angle of throat (acute angle of direct tube section and taper type contraction section) of lower part taper type contraction section is 35 °；6 top direct tube section of outer barrel
Height be 0.7m；The 5 a diameter of 150mm of spindle axial cross section maximum of baffle.Using kerosene as liquid, oil inlet quantity is
60~120L/hr；Gas phase selects nitrogen, and air inflow is 2~4Nm3/hr.Solid phase selects the aluminium oxide that grain size is 0.7~0.8mm
Microspherical catalyst, catalyst inventory (by it is static when in terms of) be reactor dischargeable capacity (disregarding end socket space) 55%~80%.
Result of the test is shown in Table 1：
1 cold model unit result of the test of table
From cold model experiment as can be seen that boiling bed hydrogenation reaction system of the present invention has good solid separation effect
Fruit, applicable operating range are wider.
Claims (10)
1. a kind of boiling bed hydrogenation reaction system, including boiling bed hydrogenation reactor and catalyst discharging system, reactor shell
(3) bottom is equipped with feed(raw material)inlet (1), and top is equipped with catalyst and adds in mouth (9), gas vent (10) and liquid outlet, reaction
Top setting gas, liquid, solid three phase separator in device cylinder (3), bottom setting gas-liquid partition tray (2), three phase separator and gas
Region between liquid distribution plate (2) is reaction zone (4), it is characterised in that：Catalyst discharging system includes the outer row pipeline of catalyst
(21) and outer row's catalyst receives and processing system (20), and one end of the outer row pipeline (21) of catalyst is from reactor shell (3)
The lower part of reaction zone (4) is stretched into lower section, and the other end is received with outer row's catalyst and processing system (20) connects；Add recycle hydrogen system
It unites (12), including circulating hydrogen compressor, the isolated hydrogen-containing gas of three phase separator flows out through gas vent (10) and through anti-
Gas phase effluent piece-rate system (11) is answered to be passed through circulating hydrogen compressor, the outlet of circulating hydrogen compressor passes through branch one respectively
(14), branch two (15) is connected with reactor feed system (22), the outer row pipeline (21) of catalyst, and control is set on branch two (15)
Valve (16) processed.
2. boiling bed hydrogenation reaction system according to claim 1, it is characterised in that：It is set in the liquid phase region of three phase separator
Liquid discharge tube line (8) is put, the outlet of liquid discharge tube line (8) is the liquid outlet of reactor shell (3), and three phase separator divides
Reaction liquid phase effluent piece-rate system (13) is passed through from outlet of the obtained liquid through liquid discharge tube line (8).
3. boiling bed hydrogenation reaction system according to claim 2, it is characterised in that：Setting reaction liquid phase effluent cycle
System, the reaction liquid phase effluent circulatory system include circulating pump (18), and entrance pipe (17) and the liquid of circulating pump (18) are discharged
Pipeline (8) connects, and the outlet of circulating pump (18) is connected by pipeline (19) with the feed(raw material)inlet (1) of reactor shell (3) bottom.
4. according to the boiling bed hydrogenation reaction system any in claims 1 to 3, it is characterised in that：The three-phase separate
Include inner cylinder (7) and outer barrel (6) from device, inner cylinder (7) and outer barrel (6) are concentric and internal diameter is different, inner cylinder (7) and outer barrel (6) it is upper,
Lower both ends are all open, and the upper end opening of outer barrel (6) is less than the upper end opening of inner cylinder (7), and the lower ending opening of outer barrel (6) is less than
The lower ending opening of inner cylinder (7)；Outer barrel (6) top is direct tube section, and outer barrel (6) lower part is a taper type contraction section, the contraction section
Lower ending opening is the lower ending opening of outer barrel (6)；There is spacing between the lower ending opening of inner cylinder (7) and outer barrel contraction section.
5. boiling bed hydrogenation reaction system according to claim 4, it is characterised in that：Three phase separator and reactor shell
(3) it is concentric setting, the outer barrel (6) of three phase separator is fixed on the inner wall of reactor shell (3) by the first support construction
On, the inner cylinder (7) of three phase separator is fixed on by the second support construction on the inner wall of outer barrel (6).
6. boiling bed hydrogenation reaction system according to claim 4, it is characterised in that：The outer barrel (6) of three phase separator
The lower section setting baffle (5) of lower ending opening.
A kind of 7. boiling bed hydrogenation technique method, it is characterised in that：Using described in any claim in claim 1~7
Boiling bed hydrogenation reaction system.
8. boiling bed hydrogenation technique method according to claim 7, it is characterised in that：Reaction raw materials are heavy or original inferior
Material oil；Catalyst is solid particle, and particle diameter is 0.6~2mm, and catalyst is using aluminium oxide as carrier, in Mo, W, Ni, Co
At least one is active component；Catalyst is in 50%~85% that reactor interior loading amount is reactor volume.
9. boiling bed hydrogenation technique method according to claim 7, it is characterised in that：In the reaction of boiling bed hydrogenation system
When hydrogenation reaction is carried out in device, between the outlet of control loop hydrogen compressor and the outer row pipeline (21) of catalyst on branch two (15)
Control valve (16) makes recycle hydrogen accomplished continuously or intermittently interior into reactor shell (3) by row pipeline outside catalyst (21).
10. boiling bed hydrogenation technique method according to claim 9, it is characterised in that：Row pipeline (21) outside catalyst
Into 5% that the cycle hydrogen amount in reactor shell (3) is global cycle hydrogen amount hereinafter, making simultaneously in the outer row pipeline (21) of catalyst
Material flow be not less than 0.1 meter per second.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109967003A (en) * | 2019-04-26 | 2019-07-05 | 河南百优福生物能源有限公司 | A kind of biomass pyrolysis liquid fluidized bed reactor and its application |
| CN110102227A (en) * | 2019-04-26 | 2019-08-09 | 河南百优福生物能源有限公司 | Biomass pyrolysis liquid fluidized bed reactor and its application |
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| CN102041084A (en) * | 2009-10-21 | 2011-05-04 | 中国石油化工股份有限公司 | Heavy hydrocarbon hydrogenation combined process |
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| CN1059164A (en) * | 1989-07-19 | 1992-03-04 | 切夫里昂研究和技术公司 | Change in the packed bed particulate method and apparatus in the operation with liquid gas feedstream counter current contact |
| CN102041084A (en) * | 2009-10-21 | 2011-05-04 | 中国石油化工股份有限公司 | Heavy hydrocarbon hydrogenation combined process |
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| CN109967003A (en) * | 2019-04-26 | 2019-07-05 | 河南百优福生物能源有限公司 | A kind of biomass pyrolysis liquid fluidized bed reactor and its application |
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